CN103623610A - Method for extracting and purifying finotoxin-1 and scallop toxin-2 from seawater - Google Patents
Method for extracting and purifying finotoxin-1 and scallop toxin-2 from seawater Download PDFInfo
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- CN103623610A CN103623610A CN201310633780.9A CN201310633780A CN103623610A CN 103623610 A CN103623610 A CN 103623610A CN 201310633780 A CN201310633780 A CN 201310633780A CN 103623610 A CN103623610 A CN 103623610A
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- methyl alcohol
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- eluent
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- dinophysistoxin
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- NGNQZCDZXSOVQU-UHFFFAOYSA-N 8,16,18,26,34,36-hexahydroxyhentetracontane-2,6,10,14,24,28,32-heptone Chemical compound CCCCCC(O)CC(O)CC(=O)CCCC(=O)CC(O)CC(=O)CCCCCC(O)CC(O)CC(=O)CCCC(=O)CC(O)CC(=O)CCCC(C)=O NGNQZCDZXSOVQU-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 101000939689 Araneus ventricosus U2-aranetoxin-Av1a Proteins 0.000 title claims abstract description 25
- 101000633673 Buthacus arenicola Beta-insect depressant toxin BaIT2 Proteins 0.000 title claims abstract description 25
- 101000654318 Centruroides noxius Beta-mammal toxin Cn2 Proteins 0.000 title claims abstract description 25
- 101001028695 Chironex fleckeri Toxin CfTX-2 Proteins 0.000 title claims abstract description 25
- 241000237509 Patinopecten sp. Species 0.000 title claims abstract description 25
- 235000020637 scallop Nutrition 0.000 title claims abstract description 25
- 239000013535 sea water Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000741 silica gel Substances 0.000 claims abstract description 7
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000004744 fabric Substances 0.000 claims abstract description 4
- 229920000728 polyester Polymers 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 96
- 239000002250 absorbent Substances 0.000 claims description 28
- 230000002745 absorbent Effects 0.000 claims description 28
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- CLBIEZBAENPDFY-HNXGFDTJSA-N dinophysistoxin 1 Chemical compound C([C@H](O1)[C@H](C)/C=C/[C@H]2CC[C@@]3(CC[C@H]4O[C@@H](C([C@@H](O)[C@@H]4O3)=C)[C@@H](O)C[C@H](C)[C@@H]3[C@@H](CC[C@@]4(O3)[C@@H](CCCO4)C)C)O2)C(C)=C[C@]21O[C@H](C[C@@](C)(O)C(O)=O)CC[C@H]2O CLBIEZBAENPDFY-HNXGFDTJSA-N 0.000 claims description 23
- DLTYQVNXVIJKAZ-UHFFFAOYSA-N dinophysistoxin-1 Natural products CC1CCC2(OCCCC2C)OC1C(O)CC(O)C3OC4CCC5(CCC(O5)C=CCC6CC(=CC7(OC(CC(C)(O)C(=O)O)CCC7O)O6)C)OC4C(O)C3=C DLTYQVNXVIJKAZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000003480 eluent Substances 0.000 claims description 18
- 238000000746 purification Methods 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920003053 polystyrene-divinylbenzene Polymers 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 239000006166 lysate Substances 0.000 claims 2
- 239000004576 sand Substances 0.000 claims 2
- 239000003463 adsorbent Substances 0.000 claims 1
- 238000012856 packing Methods 0.000 claims 1
- 241000195493 Cryptophyta Species 0.000 abstract description 5
- 235000015170 shellfish Nutrition 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 4
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000009958 sewing Methods 0.000 abstract 1
- 238000004587 chromatography analysis Methods 0.000 description 8
- 239000003053 toxin Substances 0.000 description 7
- 231100000765 toxin Toxicity 0.000 description 7
- 238000001819 mass spectrum Methods 0.000 description 6
- 239000000287 crude extract Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229960001866 silicon dioxide Drugs 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- PTKFEDGHUVZLPL-LLUYWJARSA-N Pectenotoxin 2 Chemical compound O[C@@H]1[C@H](C)CCO[C@]1(O)[C@H]1O[C@@H]2/C=C/C(/C)=C/[C@H](C)C[C@](C)(O3)CC[C@@H]3[C@](O3)(O4)CC[C@@]3(C)C[C@@H]4[C@@H](O3)C(=O)C[C@]3(C)[C@@H](O)[C@@H](O3)CC[C@@]3(O3)CCC[C@H]3[C@@H](C)C(=O)O[C@@H]2C1 PTKFEDGHUVZLPL-LLUYWJARSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 101100313763 Arabidopsis thaliana TIM22-2 gene Proteins 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- PTKFEDGHUVZLPL-UHFFFAOYSA-N Pectenotoxin 2 Natural products OC1C(C)CCOC1(O)C1OC2C=CC(C)=CC(C)CC(C)(O3)CCC3C(O3)(O4)CCC3(C)CC4C(O3)C(=O)CC3(C)C(O)C(O3)CCC3(O3)CCCC3C(C)C(=O)OC2C1 PTKFEDGHUVZLPL-UHFFFAOYSA-N 0.000 description 1
- 241000200248 Prorocentrum Species 0.000 description 1
- 208000004891 Shellfish Poisoning Diseases 0.000 description 1
- 241000719329 Trentepohlia Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000741 diarrhetic effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 210000004916 vomit Anatomy 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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Abstract
The invention relates to a method for extracting finotoxin-1 and scallop toxin-2 from seawater, which comprises the following steps: 1) sewing into an adsorption bag with 48 μm polyester mesh cloth, filling adsorption resin into the adsorption bag, sealing, and adsorbing; 2) using a glass sand core chromatographic column, firstly washing off the salt in the adsorption resin by using deionized water; 3) purifying by using a glass sand core chromatographic column filled with alumina filler with the particle size of 75-150 mu m; 4) purifying with glass sand core chromatographic column filled with reversed phase C18 silica gel to obtain mixture containing finphycotoxin-1 and scallop toxin-2. The invention has the beneficial effects that the invention can simultaneously prepare two substances of the fintoxin-1 and the scallop toxin-2, and can be used as mixed standard substances. The method is not limited by the quantity of the collected algae and shellfish, can be extracted and prepared from seawater in natural sea areas in large scale, and is simple and effective.
Description
Technical field
The present invention relates to a kind of method of extracting dinophysistoxin-1 and scallop toxin-2 from seawater.
Background technology
Research of diarrhetic shellfish poisons (Diarrhetic Shellfish Poisoning, DSP) is the fat-soluble many cyclic ethers class bioactivator by some kinds generations of red tide algae fin Trentepohlia and Prorocentrum.DSP causes that eater suffers from diarrhoea, vomits, transference cure in the common a few days, and patient can self-healing.DSP often occurs at China coast, is also one of main toxin kind of countries in the world monitoring.No matter be that toxin is monitored reliably and analyzes, still develop new toxin monitoring analysis technology, especially prepare toxin quick detection kit, all must use a large amount of toxin standard items.
China does not also have dinophysistoxin-1(Dinophysistoxin-1, DTX-1 at present) and scallop toxin-2(Pectenotoxin-2, PTX-2) technology of preparing.
Abroad, the preparation of dinophysistoxin-1 and scallop toxin-2 has two kinds of methods conventionally, and the one, from shellfish tissue, extract.But because shellfish morphological element is complicated, in extract, lipid impurity is more, purifies purification process process more complicated.Another kind is to extract from poisonous algae.Owing to producing algae more difficult cultivation under laboratory condition of dinophysistoxin-1 and scallop toxin-2, the quantity of once cultivating is also restricted, so preparation process is very difficult.
Summary of the invention
For the defect existing in prior art, the object of this invention is to provide the novel technical method that the present invention has set up a kind of extraction from natural waters seawater, separation and purification dinophysistoxin-1 and scallop toxin-2, this technology can gather in a large number dinophysistoxin-1 and scallop toxin-2 from seawater, is not gathered number quantitative limitation.Owing to adopting special macroporous absorbent resin, the toxin impurity extracting from seawater is at first less, and when further separation, purification, technology is simple.
The present invention adopts following technical scheme:
A method of extracting dinophysistoxin-1 and scallop toxin-2 from seawater, concrete steps are as follows:
1) with the polyester screen cloth that aperture is 48 μ m, be sewn into absorbent packet, in absorbent packet, pack into and take the macroporous absorbent resin that nonpolar polystyrene-divinylbenzene is matrix, sealing, by absorbent packet hang over cursory on, absorbent packet is positioned at the following 0.5～1m of seawater surface place, soaks and takes out afterwards for 7 days;
2) the each 10g of the macroporous absorbent resin in absorbent packet is proceeded to without a mark mouthful 4F piston and had in core glass chromatography column, with 50～70mL deionized water drip washing core filter post, wash away the salinity in macroporous absorbent resin, moisture positive pressure blowing in core filter post, and then add 20mL methanol-eluted fractions, with the speed of 1 per second, filter in 50ml rotary evaporation bottle; Add again 20mL methyl alcohol, repeat to extract, merge eluent in rotary evaporation bottle; Eluent is removed methyl alcohol in 40 ℃ of water-bath rotating pressure-decreasings, during to remaining 1～2mL water, then adds 5mL carrene, then centrifugal, take out dichloromethane layer, then repeat once with 5mL carrene, the carrene that merges secondary, then dries up with nitrogen, finally with the methyl alcohol of 1.0mL80%, dissolves; By above-mentioned steps, the macroporous absorbent resin in absorbent packet is repeated to multi-pass operation, obtain crude extract;
3) by 10g, through the aluminium oxide of 650 ℃ of calcinations, (chromatography is used, granularity 75～150um) pack into without a mark mouthful 4F piston and have in core glass chromatography column, liquid first with methylene chloride/methanol (volume ratio, 5/5), infiltrates, when will drain off to the greatest extent, add above-mentioned crude extract 10ml, with 20ml methylene chloride/methanol (volume ratio, 5/5) wash-out, collect eluent again, after eluent rotary evaporation is concentrated, with 5ml80% methyl alcohol dissolved residue;
4) the methyl alcohol dissolved matter after above-mentioned alumina column is processed by anti-phase C18 silica gel (particle diameter 40～60 μ m) the further purified treatment of post; The anti-phase C18 silica filler of 10g is respectively charged into without a mark mouthful 4F piston and is had in core glass chromatography column, first add 10ml100% methyl alcohol to infiltrate, when in post, methyl alcohol will drain off to the greatest extent, add again the methyl alcohol dissolved matter after the above-mentioned alumina column of 30ml is processed, with 80% methanol/water wash-out, collect eluent, concentrated rear with 2ml80% methanol/water dissolved residue, obtain the compounding substances that contains dinophysistoxin-1 and scallop toxin-2.
The invention has the beneficial effects as follows:
The present invention can prepare dinophysistoxin-1 and scallop toxin-2 two kind of material simultaneously, can be used as hybrid standard material and uses.The algae and the shellfish that are not gathered are counted quantitative limitation, can from natural waters seawater, extract in enormous quantities preparation, and method is simple, effective, and the splitter and the eluent that particularly in separation, purifying step, use, can effectively improve the effect of separation, purification.
Accompanying drawing explanation
The present invention has following accompanying drawing:
The mass spectrogram of Fig. 1 dinophysistoxin-1 standard items;
The goods figure of Fig. 2 scallop toxin-2 standard items;
The mass spectrogram of dinophysistoxin-1 that Fig. 3 alumina column obtains after processing;
The mass spectrogram of scallop toxin-2 that Fig. 4 alumina column obtains after processing;
The mass spectrogram of dinophysistoxin-1 obtaining after Fig. 5 C18 silicagel column purified treatment;
The mass spectrogram of scallop toxin-2 that obtain after Fig. 6 C18 silicagel column purified treatment.
The specific embodiment
From seawater, extract a method of preparing dinophysistoxin-1 and scallop toxin-2, concrete steps are as follows:
1) absorption: be sewn into absorbent packet with the polyester screen cloth that aperture is 48 μ m, the length of side is the square bag of 10cm * 10cm, take 100g and take the macroporous absorbent resin (HP20 that nonpolar polystyrene-divinylbenzene is matrix, Mitsubishi chemical Co., Ltd) in absorbent packet, sealing afterwards, and one jiao of absorbent packet fixedly nylon buckle.20 absorbent packets, June, hang over the cursory upper of sea area, gulf, the Huanghai Sea Lingshan, 0.5～1m place below seawater surface, soaks and takes out afterwards for 7 days;
2) the each 10g of the macroporous absorbent resin in absorbent packet is proceeded to without a mark mouthful 4F piston and has core glass chromatography column (internal diameter 22mm, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, with 50～70mL deionized water drip washing core filter post, wash away the salinity in macroporous absorbent resin, moisture positive pressure blowing in core filter post, and then add 20mL methanol-eluted fractions, with the speed of 1 per second, filter in 50ml rotary evaporation bottle; Add again 20mL methyl alcohol, repeat to extract, merge eluent in rotary evaporation bottle; Eluent is removed methyl alcohol in 40 ℃ of water-bath rotating pressure-decreasings, during to remaining 1-2mL water, then adds 5mL carrene, then centrifugal, take out dichloromethane layer, then repeat once with 5mL carrene, the carrene that merges secondary, then dries up with nitrogen, finally with the methyl alcohol of 1.0mL80%, dissolves; By above-mentioned steps, the macroporous absorbent resin in absorbent packet is repeated to multi-pass operation, obtain crude extract;
3) crude extract is purified and removes pigment impurity through alumina column.By 10g, through the aluminium oxide of 650 ℃ of calcinations, (chromatography is used, granularity 75～150 μ m, land, Shanghai is chemical reagent factory all) pack into without a mark mouthful 4F piston and have core glass chromatography column (internal diameter 22mm, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, first with methylene chloride/methanol (volume ratio, 5/5) infiltrate, when liquid will drain off to the greatest extent, add above-mentioned crude extract 10ml, then with 20ml methylene chloride/methanol (volume ratio, 5/5) wash-out, collect eluent, after eluent rotary evaporation is concentrated, with 5ml80% methyl alcohol dissolved residue.
Repeat above-mentioned purification run, merge repeatedly the methyl alcohol dissolved matter of gained;
The effect of this step is to utilize alumina column to purify to remove the pigment impurity in thick extracting toxin from seawater.
Meanwhile, get 1ml after 0.22 μ m membrane filtration, by high pressure liquid chromatography-tandem mass spectrometer (TSQ Quantum Access, U.S. Thermo Fischer Scient Inc.), analyzed.As shown in Figure 3, concentration is 106.6ng/ml to dinophysistoxin-1 mass spectrum; Scallop toxin-2 mass spectrum as shown in Figure 4 concentration is 418.1ng/ml.
4) the methyl alcohol dissolved matter after above-mentioned alumina column is processed by anti-phase C18 silica gel (particle diameter 40～60 μ m) the further purified treatment of post.The anti-phase C18 silica filler of 10g is respectively charged into without a mark mouthful 4F piston and has core glass chromatography column (internal diameter 22mm, length 200mm-300mm, Shanghai Chu Bai laboratory equipment Co., Ltd) in, first add 10ml methyl alcohol to infiltrate, when methyl alcohol will drain off to the greatest extent in post, then add the methyl alcohol dissolved matter after the above-mentioned alumina column of 30ml is processed, with 80% methanol/water wash-out, collect eluent, after eluent is concentrated, with 2ml80% methyl alcohol, dissolve, obtain the compounding substances that contains dinophysistoxin-1 and scallop toxin-2.
The effect of this step is to utilize C18 silicagel column isolation of purified to remove various non polar impurities.
Meanwhile, get 1ml after 0.22 μ m membrane filtration, by high pressure liquid chromatography-tandem mass spectrometer, analyzed, as shown in Figure 5, concentration is 24.7ng/ml to dinophysistoxin-1 mass spectrum; As shown in Figure 6, concentration is 24.5ng/ml to scallop toxin-2 mass spectrum.
By high pressure liquid chromatography-tandem mass spectrometer, analyzed, as shown in Figure 1, the mass spectrum of scallop toxin-2 standard items that concentration is 200ng/ml as shown in Figure 2 for the mass spectrum of dinophysistoxin-1 standard items that concentration is 200ng/ml.
Claims (2)
1. from seawater, extract a method for dinophysistoxin-1 and scallop toxin-2, it is characterized in that concrete steps are as follows:
1) with the polyester screen cloth that aperture is 48 μ m, be sewn into absorbent packet, pack macroporous absorbent resin in absorbent packet into, sealing, hangs over absorbent packet to be arranged at the cursory upper of sea, and absorbent packet is positioned at the following 0.5～1m of seawater surface place, soaks and takes out afterwards for 7 days;
2) use glass sand core chromatographic column, first by deionized water, wash away the salinity in polymeric adsorbent, then use methanol-eluted fractions, eluent is removed methyl alcohol at 40 ℃ of water-bath rotating pressure-decreasings, adds afterwards carrene, centrifugal, take out dichloromethane layer, utilize nitrogen to dry up, finally with 80% methyl alcohol, dissolve;
3) get step 2) the methyl alcohol lysate prepared, it is that the glass sand sandwich layer of the alumina packing of 75～150 μ m is analysed column purification and processed that granularity is equipped with in use, and eluent is methylene chloride/methanol (volume ratio is 5/5), collects eluent, after eluent rotary evaporation is concentrated, with 80% methyl alcohol dissolved residue; Described aluminium oxide is through 650 ℃ of calcinations;
4) get the methyl alcohol lysate that step 3) obtains, use the glass sand sandwich layer that anti-phase C18 silica gel is housed to analyse column purification processing, eluent is 80% methyl alcohol, collects eluent, obtains the mixture that contains dinophysistoxin-1 and scallop toxin-2.
2. the method for extracting dinophysistoxin-1 and scallop toxin-2 from seawater according to claim 1, is characterized in that the macroporous absorbent resin described in step 1) is for take the macroporous absorbent resin that nonpolar polystyrene-divinylbenzene is matrix.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198900A (en) * | 2015-09-22 | 2015-12-30 | 国家海洋环境检测中心 | Pure yessotoxin (YTX) extracting and preparing method |
| CN105561958A (en) * | 2016-03-01 | 2016-05-11 | 中国水产科学研究院黄海水产研究所 | Ionic liquid bonded silica gel for enrichment and purification of shellfish toxins and preparation method thereof |
| CN107941968A (en) * | 2017-07-21 | 2018-04-20 | 浙江大学 | It is a kind of that the method that 2 standard sample of scallop toxin is prepared in algae solution is cultivated from extensive fin algae |
| CN108469480A (en) * | 2018-03-20 | 2018-08-31 | 上海泰坦科技股份有限公司 | A kind of detection method of saxitoxin and its application |
| CN108977504A (en) * | 2018-08-06 | 2018-12-11 | 浙江海洋大学 | A kind of method that quick screening generates dinophysistoxin microbial strains |
| CN115343378A (en) * | 2021-09-06 | 2022-11-15 | 国家海洋环境监测中心 | Method for separating and purifying okadaic acid and finotoxin homologues in prorocentrum lima |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198900A (en) * | 2015-09-22 | 2015-12-30 | 国家海洋环境检测中心 | Pure yessotoxin (YTX) extracting and preparing method |
| CN105561958A (en) * | 2016-03-01 | 2016-05-11 | 中国水产科学研究院黄海水产研究所 | Ionic liquid bonded silica gel for enrichment and purification of shellfish toxins and preparation method thereof |
| CN105561958B (en) * | 2016-03-01 | 2018-05-11 | 中国水产科学研究院黄海水产研究所 | Ionic liquid bonded silica gel for enrichment and purification of shellfish toxins and preparation method thereof |
| CN107941968A (en) * | 2017-07-21 | 2018-04-20 | 浙江大学 | It is a kind of that the method that 2 standard sample of scallop toxin is prepared in algae solution is cultivated from extensive fin algae |
| CN107941968B (en) * | 2017-07-21 | 2023-07-25 | 浙江大学 | Method for preparing scallop toxin-2 standard sample from large-scale fin algae culture algae liquid |
| CN108469480A (en) * | 2018-03-20 | 2018-08-31 | 上海泰坦科技股份有限公司 | A kind of detection method of saxitoxin and its application |
| CN108977504A (en) * | 2018-08-06 | 2018-12-11 | 浙江海洋大学 | A kind of method that quick screening generates dinophysistoxin microbial strains |
| CN108977504B (en) * | 2018-08-06 | 2022-03-22 | 浙江海洋大学 | Method for rapidly screening microbial strains generating finotoxin |
| CN115343378A (en) * | 2021-09-06 | 2022-11-15 | 国家海洋环境监测中心 | Method for separating and purifying okadaic acid and finotoxin homologues in prorocentrum lima |
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| CN103623610B (en) | 2015-09-16 |
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